Star-shaped borophosphazene derivative intumescent flame retardant and preparation method thereof

A technology of intumescent flame retardant and borophosphazene, which is applied in the field of star-shaped borophosphazene derivative intumescent flame retardant and its preparation, can solve the problem of low flame retardancy and the need to further improve the flame retardant effect. problem, achieve the effect of preventing combustion, inhibiting chain reaction, and solving high toxicity

Active Publication Date: 2019-06-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecular structure of the intumescent flame retardant proposed in the prior art 201610586811.3 contains borate groups, and the flame retardancy of compounds containing borate functional groups is lower than that of compounds containing boric acid functional groups
In addition, the molecular structure of the intumescent flame retardant proposed in technology 201610586811.3 only contains two flame retardant elements, boron and nitrogen, and its flame retardant effect needs to be further improved

Method used

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  • Star-shaped borophosphazene derivative intumescent flame retardant and preparation method thereof
  • Star-shaped borophosphazene derivative intumescent flame retardant and preparation method thereof
  • Star-shaped borophosphazene derivative intumescent flame retardant and preparation method thereof

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Effect test

Embodiment 1

[0030] Embodiment 1: Preparation of star-shaped borophosphazene derivative intumescent flame retardant (HBPCP)

[0031] Step 1: Add 5.33g of hexachlorocyclotriphosphazene into 50mL of anhydrous tetrahydrofuran solution. While stirring under nitrogen atmosphere, add the above tetrahydrofuran solution dropwise to 18.34g of p-bromophenol and 7g of sodium hydroxide in 100mL of anhydrous tetrahydrofuran solution; reflux under nitrogen atmosphere for 12h;

[0032] Step 2: after the reaction, filter, distill off tetrahydrofuran, use a mixture of dichloromethane and petroleum ether with a volume ratio of 1:2 as a rinse solution, and separate with a silica gel chromatographic column to obtain intermediate product 1;

[0033] Step 3: Dissolve 10g of intermediate product 1 in 100mL of freshly steamed THF, add 12g of triisopropyl borate, add 20mL of butyl lithium dropwise under a nitrogen atmosphere at -78°C, react for 2 hours, and then gradually warm up to room temperature , overnight r...

Embodiment 2

[0041] Embodiment 2: Preparation of star-shaped borophosphazene derivative intumescent flame retardant (HBPCP)

[0042] Step 1: Add 6.95g of hexachlorocyclotriphosphazene into 75mL of anhydrous tetrahydrofuran solution. Stir under a nitrogen atmosphere, and at the same time, add the above tetrahydrofuran solution dropwise to 125 mL of anhydrous tetrahydrofuran solution of 24.2 g of p-bromophenol and 7.9 g of sodium hydroxide; reflux for 14 h under a nitrogen atmosphere;

[0043] The second step: after the reaction is finished, filter, distill off tetrahydrofuran, use a mixture of dichloromethane and petroleum ether with a volume ratio of 1:3 as a flushing solution, and separate it with a silica gel chromatographic column to obtain intermediate product 1;

[0044] Step 3: Dissolve 12g of intermediate product 1 in 100mL of freshly steamed THF, add 13g of triisopropyl borate, add 25mL of butyllithium dropwise under a nitrogen atmosphere at -78°C, react for 3 hours, and then gradu...

Embodiment 3

[0052] Embodiment 3: Preparation of star-shaped borophosphazene derivative intumescent flame retardant (HBPCP)

[0053] Step 1: Add 8.71g of hexachlorocyclotriphosphazene into 100mL of anhydrous tetrahydrofuran solution. Stir under a nitrogen atmosphere, and at the same time, add the above tetrahydrofuran solution dropwise to 150 mL of anhydrous tetrahydrofuran solution of 34.68 g of p-bromophenol and 9.87 g of sodium hydroxide; reflux for 16 h under a nitrogen atmosphere;

[0054] The second step: after the reaction is finished, filter, distill off tetrahydrofuran, use a mixture of dichloromethane and petroleum ether with a volume ratio of 1:3 as a flushing solution, and separate it with a silica gel chromatographic column to obtain intermediate product 1;

[0055] Step 3: Dissolve 14g of intermediate product 1 in 150mL of freshly steamed THF, add 15g of triisopropyl borate, add 24mL of butyllithium dropwise under a nitrogen atmosphere at -78°C, react for 4 hours, and then gr...

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Abstract

The invention discloses a starlike boron phosphazene derivative, intumescent flame retardant and a preparation method thereof. The starlike boron phosphazene derivative is hexa(4-boric acid-phenoxy)-cyclophosphazene. The preparation method includes: adding hexachlorocyclotriphosphazene into an anhydrous tetrahydrofuran solution, stirring in a nitrogen atmosphere, dropwise adding an anhydrous tetrahydrofuran solution of p-bromophenol, flowing back in a nitrogen atmosphere, filtering, steaming to remove tetrahydrofuran, flushing, and using a silica gel chromatographic column for separation to obtain an intermediate product 1; dissolving the intermediate product 1 in newly-steamed THF, adding triisopropyl borate, dropwise adding butyl lithium in a nitrogen atmosphere at minus 70-minus 78 DEG C, reacting for 1-2h, gradually increasing temperature to room temperature, and allowing reaction overnight; filtering, and steaming to remove THF to obtain an intermediate product 2; using a chromatographic column to separate flushing liquid to obtain a target product. The target product can be used as an excellent organic flame retardant.

Description

technical field [0001] The invention relates to the technical field of flame retardancy of organic polymer materials, in particular to a star-shaped borophosphazene derivative intumescent flame retardant and a preparation method thereof. Background technique [0002] There are many kinds of polymer materials and many excellent properties, which make polymer materials widely used in the national economy and people's life. However, most polymer materials are flammable, and the combustion of polymer materials will seriously threaten people's property and life safety, which hinders the further development of polymer materials in some fields. The development of flame retardants can be very good reduce such hazards. [0003] Flame retardants can be divided into inorganic flame retardants and organic flame retardants according to their properties. Inorganic flame retardants have the advantages of low smoke, low toxicity, halogen-free, good stability, and low price. Poor compatibi...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F9/6593C08K5/55C08L75/04
CPCC07F9/659C08K5/55C08L2201/02C08L75/04
Inventor刘平艾梁辉陈珊珊
OwnerSOUTH CHINA UNIV OF TECH